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In the title compound, (-)D-[CoBr(C32H38N2O4)(H2O)]·C4H8O, the benzyl­ic C atoms of the tetradentate ligand have an R,R configuration. There are two independent complex mol­ecules in the asymmetric unit, essentially of the same geometry and absolute configuration. It was possible to determine the absolute configuration based on the Flack parameter, although the crystal structure has a pseudo-center of symmetry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801003592/na6052sup1.cif
Contains datablocks abscobr, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801003592/na6052Isup2.hkl
Contains datablock I

CCDC reference: 159836

Key indicators

  • Single-crystal X-ray study
  • T = 297 K
  • Mean [sigma](C-C) = 0.021 Å
  • R factor = 0.064
  • wR factor = 0.186
  • Data-to-parameter ratio = 15.7

checkCIF results

No syntax errors found


Amber Alert Alert Level B:
PLAT_111 Alert B ADDSYM detects (pseudo) centre of symmetry ... 96 Perc Fit PLAT_112 Alert B ADDSYM detects additional (pseudo)symmetry ... ? PLAT_113 Alert B ADDSYM suggests Pseudo/New Spacegroup ........ P21/c
Yellow Alert Alert Level C:
PLAT_202 Alert C Isotropic non-H Atoms in Anion/Solvent = 10 PLAT_213 Alert C Atom O5 has ADP max/min Ratio ........... 3.10 PLAT_213 Alert C Atom C51 has ADP max/min Ratio ........... 3.50 PLAT_420 Alert C D-H Without Acceptor O(9) - H(9B) ? PLAT_702 Alert C Angle Calc 119.7(15), Rep 118.0(10), Dev. 1.13 Sigma C66 -C67 -C68 1.555 1.555 1.555 PLAT_721 Alert C Bond Calc 0.92148, Rep 0.91100, Dev. 0.01 Ang. C48 -H48A 1.555 1.555 PLAT_721 Alert C Bond Calc 0.93342, Rep 0.94400, Dev. 0.01 Ang. C70 -H70C 1.555 1.555 PLAT_722 Alert C Angle Calc 116.11, Rep 115.00, Dev. 1.11 Degree C27 -C26 -H26 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 110.09, Rep 109.00, Dev. 1.09 Degree H31B -C31 -H31C 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 119.26, Rep 118.00, Dev. 1.26 Degree C46 -C45 -H45 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 109.20, Rep 108.00, Dev. 1.20 Degree C44 -C48 -H48B 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 109.63, Rep 108.00, Dev. 1.63 Degree C44 -C48 -H48C 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 109.25, Rep 108.00, Dev. 1.25 Degree C50 -C51 -H51B 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 110.09, Rep 109.00, Dev. 1.09 Degree C53 -C61 -H61A 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 111.35, Rep 110.00, Dev. 1.35 Degree H63A -C63 -H63C 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 119.17, Rep 118.00, Dev. 1.17 Degree C67 -C66 -H66 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 118.13, Rep 117.00, Dev. 1.13 Degree C67 -C68 -H68 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 119.40, Rep 118.00, Dev. 1.40 Degree C69 -C68 -H68 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 111.32, Rep 110.00, Dev. 1.32 Degree H70B -C70 -H70C 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 111.59, Rep 110.00, Dev. 1.59 Degree H71B -C71 -H71C 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 110.10, Rep 109.00, Dev. 1.10 Degree C69 -C72 -H72A 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 109.23, Rep 108.00, Dev. 1.23 Degree C69 -C72 -H72B 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 119.39, Rep 118.00, Dev. 1.39 Degree C76 -C75 -H75 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 118.12, Rep 117.00, Dev. 1.12 Degree C78 -C77 -H77 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 110.33, Rep 109.00, Dev. 1.33 Degree C74 -C79 -H79B 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 109.13, Rep 108.00, Dev. 1.13 Degree C82 -C83 -H83C 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 110.12, Rep 109.00, Dev. 1.12 Degree H84B -C84 -H84C 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 110.24, Rep 109.00, Dev. 1.24 Degree C85 -C86 -H86A 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 109.01, Rep 108.00, Dev. 1.01 Degree C87 -C86 -H86A 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 109.23, Rep 108.00, Dev. 1.23 Degree H86A -C86 -H86B 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 112.15, Rep 111.00, Dev. 1.15 Degree C88 -C87 -H87A 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 112.30, Rep 111.00, Dev. 1.30 Degree C88 -C87 -H87B 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 109.70, Rep 108.00, Dev. 1.70 Degree H89A -C89 -H89B 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 108.07, Rep 107.00, Dev. 1.07 Degree C92 -C91 -H91A 1.555 1.555 1.555 PLAT_722 Alert C Angle Calc 117.30, Rep 116.00, Dev. 1.30 Degree C91 -C92 -H92A 1.555 1.555 1.555 General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 27.50 From the CIF: _reflns_number_total 11744 Count of symmetry unique reflns 8578 Completeness (_total/calc) 136.91% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 3166 Fraction of Friedel pairs measured 0.369 Are heavy atom types Z>Si present yes WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure
0 Alert Level A = Potentially serious problem
3 Alert Level B = Potential problem
35 Alert Level C = Please check

Comment top

The space group of the title CoIII complex, (I), is chiral since it was prepared with an optically pure tetradentate ligand. Pseudo-systematic absences h0l, l odd, were observed, which corresponds to the fact that the crystal structure has a pseudo-center of symmetry and the space group is approximately P21/c. However, both of the two independent Co complexes have the chiral ligand in an R,R configuration, as shown in Figs. 1 and 2, and there is no disorder around the asymmetric C atoms (C24, C25, C56, and C57). Although the values of the s.u.'s of coordinates are relatively high, the geometry is quite normal (Table 1).

Flack & Bernardinelli (1999) formulated the inversion-distinguishing power, which is not decreased by the pseudo-centrosymmetric arrangement of the heavy atoms if the light-atom substructure is clearly non-centrosymmetric. The title crystal is just the case and the absolute structure could be determined definitely based on Flack parameter, 0.04 (2). As seen from Fig. 3, the aromatic rings bonded at asymmetric C atoms contribute to the non-centrosymmetry.

There are intermolecular O—H···O hydrogen bonds involving the aqua ligands. The structures of the complex molecules have significant C—H···O close contacts (Table 2).

Experimental top

The chiral tetradentate ligand (-)-L [L = 1,2-bis(2,4,6-trimethylphenyl)ethane-1,2-diylbis(nitrilomethylidyne)]- bis(pentane-2,4-dione)] was derived from optically pure (+)-1,2-bis(2,4,6-trimethylphenyl)ethylenediamine, which was prepared according to the literature (Roskamp & Pedersen, 1987; Zhang, 1991). Optical resolution of the racemic diamine with (-)-mandelic acid led to optically pure (+)-diamine. The specific rotation of the ligand L and its original diamine, [α]D at 300 K, are -186° (c = 1.02, CHCl3) and +200 ° (c = 1.19, CH2Cl2), respectively. Optical purities of the ligand L and the diamine were determined using Daicel Chiralpak AD (hexane/2-propanol = 80/20, hexane/ethanol/diethylamine = 90/10/0.1, respectively). The title complex was synthesized as described previously (Yamada et al., 1999). To a solution of the ligand (-)-L in methanol were added an aqueous solution of sodium hydroxide and an aqueous solution of cobalt(II) chloride hexahydrate at 323 K under nitrogen bubbling. The cobalt(II) complex precipitated in the red–violet solution as an orange solid. This complex was oxidized to the bromocobalt(III) complex by adding bromine in CH2Cl2 under a nitrogen atmosphere. The crystals of (I) were grown from a tetrahydrofuran (THF) solution by diffusion of a little amount of hexane. The crystal specimen was sealed in a capillary to avoid efflorescence. The specific rotation [α]D of the title Co complex at 300 K is -1440° (c = 0.022, THF).

Refinement top

Friedel pairs were measured for the reflections with θ < 20°. The positional parameters of the aqua H atoms were calculated geometrically (assuming the sp2 hybridization) based on the corresponding peaks on difference syntheses. The other H-atom positional parameters were also calculated and fixed with Uiso(H) = 1.2Ueq(parent atom). The non-H atoms of THF molecules (the O15–O16 and C85–C92 atoms) were refined isotropically with restraints of C—C = 1.54 Å (s.u. 0.001 Å) and C—O = 1.43 Å (s.u. 0.001 Å). The O8, O13, C31, C63, C71 and C72 atoms were refined isotropically to avoid non-positive definite or a large max/min ratio (more than 4) of the ADP.

Computing details top

Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: TEXSAN.

Figures top
[Figure 1] Fig. 1. The structure of the complex involving the Co3 atom in (I) with displacement ellipsoids at the 50% probability level. A neighboring THF molecule is also shown.
[Figure 2] Fig. 2. The structure of the complex involving the Co4 atom in (I) with displacement ellipsoids at the 50% probability level. A neighboring THF molecule is also shown.
[Figure 3] Fig. 3. The crystal structure of (I) projected along b. C24, C25, C56 and C57 are the asymmetric C atoms in the R configuration.
(I) top
Crystal data top
[CoBr(C32H38N2O4)(H2O)]·C4H8ODx = 1.374 Mg m3
Mr = 743.62Mo Kα radiation, λ = 0.71073 Å
Monoclinic, P21Cell parameters from 25 reflections
a = 13.667 (2) Åθ = 14.6–15.0°
b = 15.046 (2) ŵ = 1.64 mm1
c = 17.764 (2) ÅT = 297 K
β = 100.32 (1)°Plate-like, brown
V = 3593.8 (8) Å30.5 × 0.3 × 0.1 mm
Z = 4
Data collection top
Rigaku AFC-7R
diffractometer
Rint = 0.046
θ–2θ scansθmax = 27.5°, θmin = 2.5°
Absorption correction: integration
(Coppens et al., 1965)
h = 018
Tmin = 0.619, Tmax = 0.854k = 1420
12278 measured reflectionsl = 2323
11744 independent reflections3 standard reflections every 150 reflections
6371 reflections with I > 2σ(I) intensity decay: 1.7%
Refinement top
Refinement on F2 w = 1/[σ2(Fo2) + (0.0754P)2 + 8.5404P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.064(Δ/σ)max = 0.020
wR(F2) = 0.186Δρmax = 0.70 e Å3
S = 1.04Δρmin = 0.60 e Å3
11744 reflectionsAbsolute structure: Flack (1983), 3169 Friedel pairs
749 parametersAbsolute structure parameter: 0.04 (2)
H-atom parameters not refined
Crystal data top
[CoBr(C32H38N2O4)(H2O)]·C4H8OV = 3593.8 (8) Å3
Mr = 743.62Z = 4
Monoclinic, P21Mo Kα radiation
a = 13.667 (2) ŵ = 1.64 mm1
b = 15.046 (2) ÅT = 297 K
c = 17.764 (2) Å0.5 × 0.3 × 0.1 mm
β = 100.32 (1)°
Data collection top
Rigaku AFC-7R
diffractometer
6371 reflections with I > 2σ(I)
Absorption correction: integration
(Coppens et al., 1965)
Rint = 0.046
Tmin = 0.619, Tmax = 0.8543 standard reflections every 150 reflections
12278 measured reflections intensity decay: 1.7%
11744 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.064H-atom parameters not refined
wR(F2) = 0.186Δρmax = 0.70 e Å3
S = 1.04Δρmin = 0.60 e Å3
11744 reflectionsAbsolute structure: Flack (1983), 3169 Friedel pairs
749 parametersAbsolute structure parameter: 0.04 (2)
Special details top

Refinement. Refinement was based on F2 against all reflections. The weighted R-factor (wR) and goodness of fit (S) were based on F2, and conventional R-factor (R) was calculated on F, with F set to zero for negative F2. The threshold expression of I > 2σ(I) was used only for calculating R-factor(gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Br10.2501 (1)0.0759 (4)0.35152 (9)0.0559 (5)
Br20.2532 (1)0.0659 (4)1.1453 (1)0.0611 (5)
Co30.1284 (1)0.0816 (4)0.4626 (1)0.0315 (5)
Co40.1249 (2)0.0805 (4)1.0379 (1)0.0391 (6)
O50.0494 (8)0.1588 (7)0.4126 (6)0.046 (3)
O60.0614 (7)0.0148 (8)0.4258 (6)0.046 (3)
O70.0605 (7)0.4315 (7)0.3980 (5)0.048 (3)
O80.1230 (7)0.2839 (8)0.4355 (6)0.06076 (4)*
O90.0226 (6)0.0892 (7)0.5567 (5)0.035 (2)
O100.0522 (7)0.1580 (8)1.0910 (6)0.046 (3)
O110.0538 (7)0.0134 (8)1.0737 (6)0.049 (3)
O120.0655 (8)0.4345 (8)1.1021 (6)0.064 (3)
O130.1265 (8)0.2818 (9)1.0793 (6)0.07646 (4)*
O140.0175 (7)0.0901 (8)0.9459 (6)0.048 (3)
O150.1797 (9)0.1483 (7)1.3017 (7)0.12530 (5)*
O160.172 (2)0.079 (1)0.187 (2)0.3024 (2)*
N170.1942 (9)0.1749 (8)0.5001 (7)0.042 (3)
N180.2087 (7)0.0085 (8)0.5117 (6)0.026 (2)
N190.1957 (7)0.1737 (8)1.0019 (6)0.027 (3)
N200.1877 (8)0.0025 (9)0.9803 (6)0.038 (3)
C210.060 (1)0.241 (1)0.4002 (9)0.045 (4)
C220.125 (1)0.2943 (9)0.4315 (8)0.034 (3)
C230.1826 (9)0.2609 (10)0.4819 (8)0.030 (3)
C240.2464 (8)0.1488 (8)0.5626 (7)0.035 (3)
C250.2869 (8)0.0535 (8)0.5439 (6)0.042 (3)
C260.209 (1)0.078 (1)0.5058 (8)0.040 (4)
C270.1507 (10)0.1328 (9)0.4623 (8)0.034 (4)
C280.082 (1)0.100 (1)0.4244 (9)0.042 (4)
C290.0092 (9)0.2699 (10)0.3465 (7)0.040 (3)
C300.130 (1)0.393 (1)0.4188 (9)0.046 (4)
C310.205 (1)0.447 (1)0.4487 (9)0.06704 (6)*
C320.3253 (9)0.2157 (9)0.5820 (8)0.031 (3)
C330.317 (1)0.2502 (9)0.6535 (9)0.040 (4)
C340.387 (1)0.305 (1)0.6719 (8)0.044 (4)
C350.470 (1)0.3336 (10)0.6200 (9)0.040 (3)
C360.4737 (10)0.3063 (10)0.5453 (8)0.043 (4)
C370.407 (1)0.2471 (9)0.5214 (9)0.040 (4)
C380.236 (1)0.2179 (10)0.7188 (8)0.065 (4)
C390.5451 (9)0.3961 (10)0.6413 (8)0.058 (4)
C400.418 (1)0.224 (1)0.4381 (8)0.050 (4)
C410.3165 (9)0.0074 (9)0.6110 (8)0.033 (3)
C420.2487 (9)0.0247 (10)0.6758 (9)0.044 (4)
C430.286 (2)0.074 (1)0.7341 (9)0.071 (5)
C440.386 (1)0.087 (1)0.729 (1)0.064 (5)
C450.454 (1)0.051 (1)0.667 (1)0.067 (5)
C460.424 (1)0.0069 (10)0.6091 (10)0.056 (4)
C470.140 (1)0.012 (1)0.6864 (9)0.068 (5)
C480.426 (2)0.136 (2)0.793 (1)0.120 (9)
C490.4994 (10)0.029 (1)0.5451 (9)0.060 (4)
C500.169 (1)0.2297 (9)0.4663 (9)0.047 (4)
C510.249 (2)0.268 (1)0.506 (1)0.095 (7)
C520.016 (1)0.150 (1)0.3792 (9)0.054 (4)
C530.059 (1)0.2420 (9)1.0984 (8)0.036 (4)
C540.1234 (10)0.296 (1)1.0628 (8)0.038 (4)
C550.192 (1)0.255 (1)1.0212 (8)0.038 (4)
C560.2799 (8)0.1383 (9)0.9665 (7)0.039 (3)
C570.2342 (8)0.0564 (8)0.9218 (6)0.036 (2)
C580.196 (1)0.082 (1)0.9880 (8)0.039 (3)
C590.151 (1)0.135 (1)1.0361 (8)0.043 (4)
C600.075 (1)0.094 (1)1.0747 (8)0.040 (4)
C610.001 (1)0.2814 (10)1.1527 (10)0.054 (5)
C620.127 (1)0.3904 (10)1.0729 (8)0.039 (4)
C630.221 (1)0.443 (2)1.063 (1)0.10463 (9)*
C640.336 (1)0.2066 (10)0.9319 (9)0.039 (3)
C650.416 (1)0.245 (1)0.9747 (9)0.054 (4)
C660.477 (1)0.304 (1)0.942 (1)0.085 (7)
C670.454 (1)0.329 (1)0.867 (1)0.063 (5)
C680.374 (1)0.296 (1)0.823 (1)0.060 (5)
C690.310 (1)0.2330 (9)0.8506 (9)0.041 (4)
C700.451 (1)0.223 (1)1.061 (1)0.072 (5)
C710.521 (1)0.392 (1)0.833 (1)0.10372 (9)*
C720.215 (1)0.214 (1)0.8034 (9)0.06748 (6)*
C730.291 (1)0.000 (1)0.8707 (8)0.047 (4)
C740.3911 (9)0.0162 (10)0.8908 (7)0.036 (3)
C750.434 (1)0.069 (1)0.837 (1)0.068 (5)
C760.378 (2)0.104 (1)0.770 (1)0.082 (7)
C770.281 (1)0.083 (1)0.7587 (10)0.072 (5)
C780.238 (2)0.0341 (10)0.8081 (9)0.063 (5)
C790.458 (1)0.0117 (10)0.960 (1)0.074 (5)
C800.430 (2)0.157 (1)0.720 (1)0.109 (8)
C810.124 (1)0.0240 (10)0.7847 (8)0.057 (4)
C820.171 (1)0.229 (1)1.0400 (8)0.043 (4)
C830.248 (1)0.266 (1)1.0023 (10)0.066 (5)
C840.019 (1)0.150 (1)1.1274 (10)0.066 (5)
C850.2803 (10)0.152 (1)1.290 (1)0.13210 (9)*
C860.324 (1)0.068 (1)1.333 (1)0.12039 (8)*
C870.242 (1)0.012 (1)1.360 (1)0.1601 (1)*
C880.151 (1)0.0587 (7)1.3136 (10)0.09850 (7)*
C890.233 (2)0.137 (1)0.222 (1)0.1557 (1)*
C900.333 (2)0.103 (2)0.177 (1)0.1864 (1)*
C910.292 (1)0.034 (1)0.127 (1)0.12957 (8)*
C920.190 (2)0.009 (1)0.156 (2)0.3464 (3)*
H9A0.03420.05130.56420.0434*
H9B0.02990.13400.59340.0434*
H14A0.01230.03750.92280.0578*
H14B0.00580.14560.92210.0578*
H230.21680.30370.50690.0357*
H240.19680.14430.60750.0415*
H250.34430.05800.50470.0495*
H260.25130.10890.53350.0474*
H29A0.00090.33230.33680.0492*
H29B0.00760.23870.29950.0492*
H29C0.07580.25820.36900.0492*
H31A0.25390.40850.46290.0832*
H31B0.23500.48690.41070.0832*
H31C0.17300.47880.49250.0832*
H340.37780.32600.72330.0527*
H360.52570.32940.50710.0506*
H38A0.20080.26800.74300.0792*
H38B0.19110.18020.69910.0792*
H38C0.26600.18660.75490.0792*
H39A0.60970.37220.62800.0712*
H39B0.54220.45160.61500.0712*
H39C0.53060.40750.69510.0712*
H40A0.36860.18220.43150.0622*
H40B0.41430.27500.40920.0622*
H40C0.48250.19630.42260.0622*
H430.24150.09740.77630.0844*
H450.52260.05960.66590.0824*
H47A0.11770.01860.73300.0804*
H47B0.12450.02150.64490.0804*
H47C0.10850.06850.68800.0804*
H48A0.37540.15720.83000.1496*
H48B0.46780.18560.77090.1496*
H48C0.46900.09700.81530.1496*
H49A0.53780.01900.52060.0751*
H49B0.46680.05850.50960.0751*
H49C0.54180.06940.56500.0751*
H51A0.22010.30810.54470.1114*
H51B0.29670.29940.46930.1114*
H51C0.28200.22170.52760.1114*
H52A0.05220.14090.40290.0631*
H52B0.02530.12700.32860.0631*
H52C0.03100.21070.37860.0631*
H550.24120.29271.00660.0452*
H560.32620.11451.00810.0465*
H570.17880.07900.88750.0429*
H580.23710.11120.95800.0473*
H61A0.00670.34351.15440.0654*
H61B0.07030.26751.13460.0654*
H61C0.01850.25621.20180.0654*
H63A0.26320.40681.04000.1219*
H63B0.20040.49331.02990.1219*
H63C0.25330.46421.11070.1219*
H660.53440.32820.97330.1004*
H680.36000.31380.77150.0726*
H70A0.40420.18161.07630.0902*
H70B0.51420.19561.06790.0902*
H70C0.45250.27481.09010.0902*
H71A0.57510.40810.87310.1249*
H71B0.54800.36060.79460.1249*
H71C0.48590.44140.81320.1249*
H72A0.17700.26610.79480.0817*
H72B0.22540.18950.75590.0817*
H72C0.18110.17100.82890.0817*
H750.50380.07930.84810.0800*
H770.23960.10470.71330.0866*
H79A0.48620.03920.98830.0867*
H79B0.51010.04710.94740.0867*
H79C0.42220.04530.99180.0867*
H80A0.45720.20830.74620.1295*
H80B0.38090.17640.67600.1295*
H80C0.47820.12320.70240.1295*
H81A0.09880.01070.82170.0680*
H81B0.10840.00440.73620.0680*
H81C0.09320.08110.78150.0680*
H83A0.29850.29151.03920.0803*
H83B0.21930.31010.96680.0803*
H83C0.27510.21990.97570.0803*
H84A0.03690.12891.17870.0821*
H84B0.04940.14601.11070.0821*
H84C0.04020.21091.12630.0821*
H85A0.31370.20361.31260.1543*
H85B0.28510.14931.23760.1543*
H86A0.37210.08381.37590.1431*
H86B0.35460.03191.29920.1431*
H87A0.24420.01731.41370.1893*
H87B0.24510.04901.34700.1893*
H88A0.13060.02971.26580.1172*
H88B0.09720.05841.34120.1172*
H89A0.22600.12770.27540.1870*
H89B0.22210.19790.21210.1870*
H90A0.37250.07540.21000.2207*
H90B0.37080.14810.14830.2207*
H91A0.33940.01180.11590.1541*
H91B0.28620.06420.08010.1541*
H92A0.15300.02730.11910.4292*
H92B0.19030.05530.19310.4292*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Br10.071 (1)0.0512 (10)0.045 (1)0.0017 (10)0.0101 (9)0.0009 (9)
Br20.086 (1)0.052 (1)0.043 (1)0.0007 (9)0.0052 (9)0.0064 (8)
Co30.037 (1)0.0207 (9)0.040 (1)0.0028 (9)0.0156 (9)0.0014 (9)
Co40.052 (1)0.029 (1)0.039 (1)0.0005 (10)0.016 (1)0.0021 (9)
O50.069 (7)0.009 (5)0.067 (7)0.002 (4)0.033 (6)0.002 (4)
O60.054 (6)0.039 (6)0.052 (7)0.002 (5)0.030 (5)0.009 (5)
O70.062 (7)0.032 (6)0.054 (7)0.006 (5)0.024 (5)0.012 (5)
O90.039 (5)0.024 (5)0.048 (6)0.002 (4)0.020 (4)0.001 (4)
O100.039 (6)0.060 (7)0.045 (7)0.003 (5)0.022 (5)0.004 (5)
O110.057 (6)0.030 (6)0.066 (7)0.004 (5)0.024 (5)0.009 (5)
O120.083 (8)0.037 (6)0.075 (8)0.020 (6)0.023 (7)0.019 (6)
O140.036 (5)0.043 (6)0.062 (7)0.006 (5)0.000 (5)0.007 (5)
N170.055 (8)0.029 (7)0.051 (8)0.004 (6)0.037 (7)0.007 (6)
N180.024 (5)0.016 (5)0.039 (6)0.000 (4)0.011 (4)0.001 (4)
N190.030 (6)0.024 (6)0.026 (6)0.001 (5)0.001 (5)0.002 (5)
N200.040 (6)0.033 (6)0.044 (7)0.012 (5)0.010 (5)0.000 (5)
C210.037 (8)0.048 (10)0.051 (10)0.023 (7)0.014 (7)0.024 (8)
C220.047 (9)0.012 (6)0.042 (8)0.003 (6)0.008 (7)0.002 (6)
C230.020 (6)0.029 (8)0.042 (9)0.005 (5)0.009 (6)0.007 (6)
C240.038 (7)0.012 (5)0.058 (8)0.000 (5)0.016 (6)0.001 (5)
C250.050 (7)0.033 (6)0.048 (7)0.010 (5)0.023 (6)0.011 (5)
C260.045 (8)0.039 (9)0.036 (8)0.010 (7)0.007 (6)0.014 (7)
C270.029 (8)0.023 (7)0.05 (1)0.000 (6)0.007 (7)0.004 (7)
C280.06 (1)0.020 (7)0.039 (9)0.016 (7)0.003 (8)0.006 (6)
C290.039 (7)0.050 (8)0.029 (7)0.011 (6)0.001 (6)0.001 (6)
C300.06 (1)0.044 (9)0.032 (8)0.006 (8)0.011 (7)0.004 (7)
C320.025 (6)0.017 (6)0.054 (9)0.001 (5)0.019 (6)0.003 (6)
C330.042 (8)0.020 (6)0.055 (9)0.001 (6)0.001 (7)0.003 (6)
C340.059 (9)0.039 (8)0.038 (8)0.004 (7)0.023 (8)0.008 (7)
C350.046 (8)0.034 (7)0.045 (8)0.000 (6)0.018 (7)0.003 (6)
C360.033 (8)0.030 (7)0.059 (9)0.001 (6)0.007 (6)0.005 (6)
C370.049 (8)0.011 (6)0.06 (1)0.008 (6)0.018 (8)0.003 (6)
C380.08 (1)0.059 (8)0.046 (8)0.012 (7)0.010 (7)0.010 (7)
C390.040 (7)0.061 (8)0.078 (10)0.026 (6)0.024 (7)0.012 (7)
C400.046 (8)0.056 (8)0.044 (8)0.001 (6)0.008 (6)0.005 (7)
C410.041 (7)0.021 (6)0.038 (7)0.006 (5)0.012 (6)0.004 (5)
C420.037 (7)0.038 (8)0.07 (1)0.003 (6)0.036 (7)0.001 (7)
C430.13 (2)0.032 (9)0.050 (10)0.001 (10)0.03 (1)0.004 (7)
C440.08 (1)0.039 (8)0.08 (1)0.001 (8)0.05 (1)0.016 (8)
C450.062 (10)0.059 (10)0.09 (1)0.004 (8)0.037 (9)0.016 (9)
C460.055 (9)0.031 (7)0.09 (1)0.020 (6)0.036 (8)0.002 (7)
C470.08 (1)0.060 (9)0.07 (1)0.010 (8)0.032 (8)0.029 (8)
C480.13 (2)0.13 (2)0.12 (2)0.02 (1)0.07 (1)0.07 (2)
C490.044 (8)0.065 (9)0.074 (10)0.002 (7)0.014 (7)0.012 (7)
C500.07 (1)0.016 (7)0.051 (10)0.013 (7)0.001 (8)0.008 (6)
C510.11 (2)0.018 (8)0.16 (2)0.009 (9)0.05 (1)0.016 (10)
C520.07 (1)0.051 (10)0.047 (9)0.010 (8)0.021 (8)0.014 (8)
C530.044 (9)0.019 (7)0.046 (9)0.004 (6)0.010 (7)0.015 (6)
C540.032 (8)0.040 (9)0.042 (9)0.006 (6)0.011 (7)0.008 (7)
C550.050 (9)0.037 (9)0.031 (8)0.003 (7)0.014 (7)0.000 (7)
C560.032 (7)0.040 (7)0.048 (8)0.008 (5)0.015 (6)0.005 (6)
C570.046 (6)0.032 (5)0.036 (6)0.004 (5)0.020 (5)0.009 (5)
C580.055 (8)0.021 (7)0.043 (8)0.004 (7)0.019 (7)0.006 (7)
C590.042 (9)0.044 (10)0.04 (1)0.011 (8)0.003 (8)0.010 (8)
C600.042 (8)0.046 (10)0.029 (8)0.002 (7)0.000 (7)0.006 (7)
C610.057 (8)0.019 (6)0.10 (1)0.005 (6)0.057 (9)0.001 (6)
C620.047 (9)0.031 (8)0.038 (8)0.018 (7)0.007 (7)0.001 (6)
C640.049 (8)0.020 (6)0.049 (8)0.002 (6)0.013 (7)0.007 (6)
C650.06 (1)0.06 (1)0.05 (1)0.004 (9)0.010 (9)0.006 (8)
C660.029 (9)0.06 (1)0.16 (2)0.010 (9)0.02 (1)0.05 (1)
C670.06 (1)0.044 (9)0.09 (1)0.007 (8)0.03 (1)0.020 (9)
C680.07 (1)0.049 (10)0.07 (1)0.005 (8)0.029 (9)0.021 (9)
C690.047 (8)0.022 (6)0.055 (9)0.001 (6)0.014 (7)0.017 (6)
C700.07 (1)0.07 (1)0.08 (1)0.019 (8)0.004 (8)0.018 (9)
C730.08 (1)0.029 (7)0.038 (8)0.009 (7)0.021 (7)0.001 (6)
C740.038 (8)0.039 (7)0.033 (7)0.001 (6)0.011 (6)0.003 (5)
C750.047 (8)0.043 (8)0.12 (1)0.022 (7)0.029 (9)0.034 (10)
C760.13 (2)0.042 (9)0.09 (2)0.022 (10)0.06 (1)0.001 (9)
C770.07 (1)0.09 (1)0.07 (1)0.01 (1)0.040 (10)0.00 (1)
C780.14 (2)0.021 (7)0.040 (8)0.002 (8)0.041 (9)0.003 (6)
C790.08 (1)0.034 (7)0.11 (1)0.013 (7)0.03 (1)0.003 (8)
C800.19 (2)0.06 (1)0.10 (2)0.02 (1)0.09 (2)0.010 (10)
C810.079 (10)0.041 (8)0.056 (9)0.018 (7)0.026 (8)0.015 (7)
C820.040 (9)0.07 (1)0.018 (7)0.014 (8)0.003 (6)0.001 (7)
C830.09 (1)0.049 (10)0.063 (10)0.005 (9)0.015 (9)0.021 (8)
C840.09 (1)0.06 (1)0.06 (1)0.045 (9)0.029 (10)0.002 (9)
Geometric parameters (Å, º) top
Br1—Co32.345 (2)C50—C511.52 (3)
Br2—Co42.359 (3)C51—H51A0.944
Co3—O51.91 (1)C51—H51B0.964
Co3—O61.89 (1)C51—H51C0.942
Co3—O92.007 (8)C52—H52A0.961
Co3—N171.85 (1)C52—H52B0.948
Co3—N181.88 (1)C52—H52C0.941
Co4—O101.89 (1)C53—C541.43 (2)
Co4—O111.89 (1)C53—C611.50 (2)
Co4—O141.997 (9)C54—C551.43 (2)
Co4—N191.88 (1)C54—C621.43 (2)
Co4—N201.87 (1)C55—H550.948
O5—C211.26 (2)C56—C571.54 (2)
O6—C281.31 (2)C56—C641.49 (2)
O7—C301.22 (2)C56—H560.952
O8—C501.22 (2)C57—C731.55 (2)
O9—H9A0.953C57—H570.946
O9—H9B0.956C58—C591.39 (2)
O10—C531.27 (2)C58—H580.948
O11—C601.25 (2)C59—C601.48 (2)
O12—C621.25 (2)C59—C821.43 (2)
O13—C821.29 (2)C60—C841.55 (2)
O14—H14A0.950C61—H61A0.940
O14—H14B0.964C61—H61B0.964
O15—C851.43 (2)C61—H61C0.945
O15—C881.43 (2)C62—C631.55 (3)
O16—C891.43 (4)C63—H63A0.940
O16—C921.43 (3)C63—H63B0.962
N17—C231.35 (2)C63—H63C0.944
N17—C241.48 (2)C64—C651.34 (2)
N18—C251.46 (2)C64—C691.48 (2)
N18—C261.30 (2)C65—C661.41 (3)
N19—C551.28 (2)C65—C701.55 (2)
N19—C561.50 (2)C66—C671.38 (3)
N20—C571.54 (2)C66—H660.946
N20—C581.29 (2)C67—C681.32 (2)
C21—C221.39 (2)C67—C711.50 (3)
C21—C291.52 (2)C68—C691.43 (2)
C22—C231.39 (2)C68—H680.946
C22—C301.50 (2)C69—C721.45 (2)
C23—H230.951C70—H70A0.959
C24—C251.55 (2)C70—H70B0.947
C24—C321.56 (2)C70—H70C0.944
C24—H240.952C71—H71A0.957
C25—C411.50 (2)C71—H71B0.961
C25—H250.953C71—H71C0.926
C26—C271.46 (2)C72—H72A0.938
C26—H260.947C72—H72B0.954
C27—C281.34 (2)C72—H72C0.953
C27—C501.48 (2)C73—C741.37 (2)
C28—C521.51 (2)C73—C781.32 (2)
C29—H29A0.957C74—C751.44 (2)
C29—H29B0.951C74—C791.46 (2)
C29—H29C0.942C75—C761.41 (3)
C30—C311.48 (2)C75—H750.955
C31—H31A0.949C76—C771.34 (3)
C31—H31B0.944C76—C801.47 (3)
C31—H31C0.952C77—C781.36 (3)
C32—C331.36 (2)C77—H770.958
C32—C371.48 (2)C78—C811.54 (3)
C33—C341.35 (2)C79—H79A0.958
C33—C381.53 (2)C79—H79B0.952
C34—C351.40 (2)C79—H79C0.950
C34—H340.951C80—H80A0.938
C35—C361.38 (2)C80—H80B0.977
C35—C391.50 (2)C80—H80C0.927
C36—C371.39 (2)C81—H81A0.952
C36—H360.955C81—H81B0.951
C37—C401.50 (2)C81—H81C0.953
C38—H38A0.953C82—C831.46 (2)
C38—H38B0.949C83—H83A0.945
C38—H38C0.946C83—H83B0.948
C39—H39A0.942C83—H83C0.954
C39—H39B0.961C84—H84A0.953
C39—H39C0.955C84—H84B0.936
C40—H40A0.946C84—H84C0.962
C40—H40B0.931C85—C861.54 (2)
C40—H40C0.967C85—H85A0.954
C41—C421.43 (2)C85—H85B0.943
C41—C461.48 (2)C86—C871.54 (3)
C42—C431.44 (2)C86—H86A0.952
C42—C471.48 (2)C86—H86B0.954
C43—C441.37 (3)C87—C881.54 (2)
C43—H430.940C87—H87A0.951
C44—C451.41 (2)C87—H87B0.948
C44—C481.54 (3)C88—H88A0.950
C45—C461.35 (3)C88—H88B0.954
C45—H450.948C89—C901.54 (3)
C46—C491.49 (2)C89—H89A0.952
C47—H47A0.949C89—H89B0.953
C47—H47B0.949C90—C911.54 (3)
C47—H47C0.948C90—H90A0.960
C48—H48A0.911C90—H90B0.939
C48—H48B0.979C91—C921.54 (3)
C48—H48C0.968C91—H91A0.946
C49—H49A0.945C91—H91B0.955
C49—H49B0.948C92—H92A0.939
C49—H49C0.955C92—H92B0.961
Br1—Co3—O590.3 (3)H52A—C52—H52B108
Br1—Co3—O689.7 (3)H52A—C52—H52C109
Br1—Co3—O9178.6 (4)H52B—C52—H52C110
Br1—Co3—N1790.7 (4)O10—C53—C54124 (1)
Br1—Co3—N1889.1 (3)O10—C53—C61115 (1)
O5—Co3—O687.5 (5)C54—C53—C61120 (1)
O5—Co3—O988.3 (4)C53—C54—C55119 (1)
O5—Co3—N1793.3 (6)C53—C54—C62121 (1)
O5—Co3—N18178.3 (5)C55—C54—C62118 (1)
O6—Co3—O990.6 (4)N19—C55—C54127 (1)
O6—Co3—N17179.1 (6)N19—C55—H55115
O6—Co3—N1894.1 (5)C54—C55—H55116
O9—Co3—N1789.0 (5)N19—C56—C57103.3 (9)
O9—Co3—N1892.3 (4)N19—C56—C64114 (1)
N17—Co3—N1885.1 (5)N19—C56—H56105
Br2—Co4—O1092.0 (3)C57—C56—C64122 (1)
Br2—Co4—O1190.6 (3)C57—C56—H56104
Br2—Co4—O14178.6 (4)C64—C56—H56105
Br2—Co4—N1989.5 (3)N20—C57—C56104.5 (9)
Br2—Co4—N2092.1 (3)N20—C57—C73114 (1)
O10—Co4—O1186.9 (5)N20—C57—H57104.2
O10—Co4—O1489.3 (4)C56—C57—C73122 (1)
O10—Co4—N1993.4 (6)C56—C57—H57104
O10—Co4—N20175.6 (4)C73—C57—H57104.4
O11—Co4—O1489.0 (4)N20—C58—C59126 (1)
O11—Co4—N19179.7 (5)N20—C58—H58116
O11—Co4—N2091.6 (6)C59—C58—H58116
O14—Co4—N1990.9 (5)C58—C59—C60117 (1)
O14—Co4—N2086.5 (5)C58—C59—C82119 (1)
N19—Co4—N2088.1 (5)C60—C59—C82122 (1)
Co3—O5—C21128 (1)O11—C60—C59125 (1)
Co3—O6—C28129 (1)O11—C60—C84113 (1)
Co3—O9—H9A122.0C59—C60—C84120 (1)
Co3—O9—H9B117.4C53—C61—H61A109
H9A—O9—H9B120.5C53—C61—H61B108
Co4—O10—C53129 (1)C53—C61—H61C109
Co4—O11—C60127 (1)H61A—C61—H61B109
Co4—O14—H14A119.2H61A—C61—H61C110
Co4—O14—H14B123.9H61B—C61—H61C108
H14A—O14—H14B116.8O12—C62—C54124 (1)
C85—O15—C88110 (1)O12—C62—C63114 (1)
C89—O16—C92130 (2)C54—C62—C63120 (1)
Co3—N17—C23123 (1)C62—C63—H63A109
Co3—N17—C24113.6 (9)C62—C63—H63B108
C23—N17—C24121 (1)C62—C63—H63C109
Co3—N18—C25116.1 (8)H63A—C63—H63B109
Co3—N18—C26122 (1)H63A—C63—H63C110
C25—N18—C26119 (1)H63B—C63—H63C108
Co4—N19—C55125 (1)C56—C64—C65119 (1)
Co4—N19—C56110.9 (8)C56—C64—C69122 (1)
C55—N19—C56121 (1)C65—C64—C69117 (1)
Co4—N20—C57109.0 (9)C64—C65—C66121 (1)
Co4—N20—C58127 (1)C64—C65—C70122 (1)
C57—N20—C58123 (1)C66—C65—C70116 (1)
O5—C21—C22124 (1)C65—C66—C67121 (1)
O5—C21—C29109 (1)C65—C66—H66119
C22—C21—C29126 (1)C67—C66—H66118
C21—C22—C23121 (1)C66—C67—C68118 (1)
C21—C22—C30121 (1)C66—C67—C71120 (1)
C23—C22—C30116 (1)C68—C67—C71120 (1)
N17—C23—C22127 (1)C67—C68—C69123 (1)
N17—C23—H23116C67—C68—H68117
C22—C23—H23116C69—C68—H68118
N17—C24—C25106.6 (10)C64—C69—C68116 (1)
N17—C24—C32116 (1)C64—C69—C72123 (1)
N17—C24—H24106C68—C69—C72118 (1)
C25—C24—C32114.2 (10)C65—C70—H70A108
C25—C24—H24106C65—C70—H70B109
C32—C24—H24106C65—C70—H70C109
N18—C25—C24104.7 (9)H70A—C70—H70B108
N18—C25—C41114.7 (10)H70A—C70—H70C109
N18—C25—H25108H70B—C70—H70C110
C24—C25—C41113.2 (10)C67—C71—H71A108
C24—C25—H25107.8C67—C71—H71B108
C41—C25—H25108C67—C71—H71C110
N18—C26—C27127 (1)H71A—C71—H71B108
N18—C26—H26116H71A—C71—H71C111
C27—C26—H26115H71B—C71—H71C110
C26—C27—C28123 (1)C69—C72—H72A109
C26—C27—C50114 (1)C69—C72—H72B108
C28—C27—C50121 (1)C69—C72—H72C108
O6—C28—C27121 (1)H72A—C72—H72B110
O6—C28—C52110 (1)H72A—C72—H72C110
C27—C28—C52128 (1)H72B—C72—H72C108
C21—C29—H29A109C57—C73—C74121 (1)
C21—C29—H29B109C57—C73—C78116 (1)
C21—C29—H29C109C74—C73—C78121 (1)
H29A—C29—H29B108C73—C74—C75115 (1)
H29A—C29—H29C109C73—C74—C79127 (1)
H29B—C29—H29C110C75—C74—C79116 (1)
O7—C30—C22120 (1)C74—C75—C76123 (1)
O7—C30—C31118 (1)C74—C75—H75117
C22—C30—C31120 (1)C76—C75—H75118
C30—C31—H31A109C75—C76—C77113 (1)
C30—C31—H31B109C75—C76—C80118 (1)
C30—C31—H31C108C77—C76—C80127 (1)
H31A—C31—H31B110C76—C77—C78124 (1)
H31A—C31—H31C109C76—C77—H77117
H31B—C31—H31C109C78—C77—H77117
C24—C32—C33120 (1)C73—C78—C77120 (1)
C24—C32—C37120 (1)C73—C78—C81124 (1)
C33—C32—C37119 (1)C77—C78—C81114 (1)
C32—C33—C34120 (1)C74—C79—H79A110
C32—C33—C38121 (1)C74—C79—H79B109
C34—C33—C38117 (1)C74—C79—H79C110
C33—C34—C35123 (1)H79A—C79—H79B108
C33—C34—H34117H79A—C79—H79C108
C35—C34—H34118H79B—C79—H79C109
C34—C35—C36115 (1)C76—C80—H80A109
C34—C35—C39122 (1)C76—C80—H80B107
C36—C35—C39121 (1)C76—C80—H80C110
C35—C36—C37124 (1)H80A—C80—H80B108
C35—C36—H36118H80A—C80—H80C112
C37—C36—H36117H80B—C80—H80C109
C32—C37—C36115 (1)C78—C81—H81A109
C32—C37—C40124 (1)C78—C81—H81B109
C36—C37—C40119 (1)C78—C81—H81C109
C33—C38—H38A109H81A—C81—H81B109
C33—C38—H38B109H81A—C81—H81C109
C33—C38—H38C109H81B—C81—H81C109
H38A—C38—H38B109O13—C82—C59122 (1)
H38A—C38—H38C109O13—C82—C83117 (1)
H38B—C38—H38C109C59—C82—C83120 (1)
C35—C39—H39A110C82—C83—H83A109
C35—C39—H39B109C82—C83—H83B109
C35—C39—H39C109C82—C83—H83C108
H39A—C39—H39B109H83A—C83—H83B110
H39A—C39—H39C109H83A—C83—H83C109
H39B—C39—H39C108H83B—C83—H83C109
C37—C40—H40A109C60—C84—H84A109
C37—C40—H40B110C60—C84—H84B110
C37—C40—H40C107C60—C84—H84C108
H40A—C40—H40B111H84A—C84—H84B110
H40A—C40—H40C108H84A—C84—H84C108
H40B—C40—H40C109H84B—C84—H84C109
C25—C41—C42124 (1)O15—C85—C86101 (1)
C25—C41—C46117 (1)O15—C85—H85A111
C42—C41—C46117 (1)O15—C85—H85B112
C41—C42—C43119 (1)C86—C85—H85A110
C41—C42—C47123 (1)C86—C85—H85B111
C43—C42—C47116 (1)H85A—C85—H85B109
C42—C43—C44120 (1)C85—C86—C87111 (1)
C42—C43—H43120C85—C86—H86A109
C44—C43—H43119C85—C86—H86B109
C43—C44—C45120 (1)C87—C86—H86A108
C43—C44—C48119 (1)C87—C86—H86B108
C45—C44—C48119 (1)H86A—C86—H86B108
C44—C45—C46122 (1)C86—C87—C8898 (1)
C44—C45—H45118C86—C87—H87A112
C46—C45—H45118C86—C87—H87B112
C41—C46—C45119 (1)C88—C87—H87A111
C41—C46—C49120 (1)C88—C87—H87B111
C45—C46—C49119 (1)H87A—C87—H87B109
C42—C47—H47A109O15—C88—C87106 (1)
C42—C47—H47B109O15—C88—H88A110
C42—C47—H47C109O15—C88—H88B109
H47A—C47—H47B109C87—C88—H88A110
H47A—C47—H47C109C87—C88—H88B110
H47B—C47—H47C109H88A—C88—H88B109
C44—C48—H48A112O16—C89—C9096 (1)
C44—C48—H48B108O16—C89—H89A112
C44—C48—H48C108O16—C89—H89B112
H48A—C48—H48B110C90—C89—H89A113
H48A—C48—H48C111C90—C89—H89B112
H48B—C48—H48C105H89A—C89—H89B108
C46—C49—H49A109C89—C90—C9197 (1)
C46—C49—H49B109C89—C90—H90A111
C46—C49—H49C109C89—C90—H90B112
H49A—C49—H49B110C91—C90—H90A111
H49A—C49—H49C109C91—C90—H90B113
H49B—C49—H49C109H90A—C90—H90B109
O8—C50—C27122 (1)C90—C91—C92119 (2)
O8—C50—C51115 (1)C90—C91—H91A107
C27—C50—C51122 (1)C90—C91—H91B106
C50—C51—H51A109C92—C91—H91A107
C50—C51—H51B108C92—C91—H91B106
C50—C51—H51C110H91A—C91—H91B109
H51A—C51—H51B108O16—C92—C9180 (1)
H51A—C51—H51C110O16—C92—H92A117
H51B—C51—H51C109O16—C92—H92B115
C28—C52—H52A108C91—C92—H92A116
C28—C52—H52B109C91—C92—H92B115
C28—C52—H52C109H92A—C92—H92B109
Co3—N17—C24—C2535 (1)N19—C56—C57—N2051 (1)
Co3—N17—C24—C32164.3 (8)N19—C56—C57—C73175 (1)
Co3—N18—C25—C2427 (1)N19—C56—C64—C6590 (1)
Co3—N18—C25—C41152.3 (8)N20—C57—C56—C64177 (1)
Co4—N19—C56—C5740.6 (10)N20—C57—C73—C7491 (1)
Co4—N19—C56—C64176.3 (8)N20—C57—C73—C7885 (1)
Co4—N20—C57—C5641.5 (9)C24—C25—C41—C4271 (1)
Co4—N20—C57—C73178.8 (8)C24—C25—C41—C46109 (1)
N17—C24—C25—N1838 (1)C25—C24—C32—C33113 (1)
N17—C24—C25—C41163.8 (10)C25—C24—C32—C3770 (1)
N17—C24—C32—C33121 (1)C56—C57—C73—C7437 (1)
N17—C24—C32—C3754 (1)C56—C57—C73—C78145 (1)
N18—C25—C24—C32168.0 (10)C57—C56—C64—C65143 (1)
N18—C25—C41—C4248 (1)C57—C56—C64—C6935 (1)
N18—C25—C41—C46130 (1)C64—C56—C57—C7344 (1)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O9—H9A···O7i0.951.942.69 (2)135
O9—H9B···O8ii0.962.562.74 (2)91
O14—H14A···O12iii0.951.732.67 (2)169
O14—H14B···O13iv0.961.972.73 (2)134
C40—H40A···N170.942.483.15 (2)128
C47—H47B···N180.952.453.09 (2)125
C29—H29A···O70.962.112.82 (2)130
C52—H52C···O80.942.072.78 (2)132
C47—H47B···O90.952.493.40 (2)159
C61—H61A···O120.941.912.69 (2)139
C84—H84C···O130.961.892.70 (2)139
C40—H40A···Br10.942.833.72 (2)157
C56—H56···Br20.952.893.44 (1)118
C68—H68···Br1i0.942.933.78 (2)151
Symmetry codes: (i) x, y+1/2, z+1; (ii) x, y1/2, z+1; (iii) x, y1/2, z+2; (iv) x, y+1/2, z+2.

Experimental details

Crystal data
Chemical formula[CoBr(C32H38N2O4)(H2O)]·C4H8O
Mr743.62
Crystal system, space groupMonoclinic, P21
Temperature (K)297
a, b, c (Å)13.667 (2), 15.046 (2), 17.764 (2)
β (°) 100.32 (1)
V3)3593.8 (8)
Z4
Radiation typeMo Kα
µ (mm1)1.64
Crystal size (mm)0.5 × 0.3 × 0.1
Data collection
DiffractometerRigaku AFC-7R
diffractometer
Absorption correctionIntegration
(Coppens et al., 1965)
Tmin, Tmax0.619, 0.854
No. of measured, independent and
observed [I > 2σ(I)] reflections
12278, 11744, 6371
Rint0.046
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.064, 0.186, 1.04
No. of reflections11744
No. of parameters749
No. of restraints?
H-atom treatmentH-atom parameters not refined
Δρmax, Δρmin (e Å3)0.70, 0.60
Absolute structureFlack (1983), 3169 Friedel pairs
Absolute structure parameter0.04 (2)

Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993), MSC/AFC Diffractometer Control Software, TEXSAN (Molecular Structure Corporation, 1999), SIR92 (Altomare et al., 1994), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), TEXSAN.

Selected geometric parameters (Å, º) top
Br1—Co32.345 (2)Co3—N181.88 (1)
Br2—Co42.359 (3)Co4—O101.89 (1)
Co3—O51.91 (1)Co4—O111.89 (1)
Co3—O61.89 (1)Co4—O141.997 (9)
Co3—O92.007 (8)Co4—N191.88 (1)
Co3—N171.85 (1)Co4—N201.87 (1)
Br1—Co3—O9178.6 (4)Br2—Co4—O14178.6 (4)
N17—C24—C25—N1838 (1)N19—C56—C57—N2051 (1)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O9—H9A···O7i0.951.942.69 (2)135
O9—H9B···O8ii0.962.562.74 (2)91
O14—H14A···O12iii0.951.732.67 (2)169
O14—H14B···O13iv0.961.972.73 (2)134
C40—H40A···N170.942.483.15 (2)128
C47—H47B···N180.952.453.09 (2)125
C29—H29A···O70.962.112.82 (2)130
C52—H52C···O80.942.072.78 (2)132
C61—H61A···O120.941.912.69 (2)139
C84—H84C···O130.961.892.70 (2)139
Symmetry codes: (i) x, y+1/2, z+1; (ii) x, y1/2, z+1; (iii) x, y1/2, z+2; (iv) x, y+1/2, z+2.
 

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